IS 6887:2005 ISO 1567:1999 WF??fkTm n <-d m!? ~+~ -@H G-T=il $ fa-q 3m-1-? diRfw!- Indian Standard DENTISTRY -- DENTURE (Second BASE POLYMERS Revision ) ICS 11.060.10 0 BIS 2005 BUREAU MANAK OF BHAVAN, 9 NEW INDIAN BAHADUR DELHI STANDARDS SHAH 110002 ZAFAR MARG June 2005 Price Group 11 Dentistry Sectional Committee, MGP 47 NATIONAL FOREWORD This Indian Standard (Second Revision) which is identical with ISO 1567:1999 `Dentistry -- Denture base polymers' with one amendment issued by the International Organization for Standardization (ISO) was adopted by the Bureau of Indian Standards on the recommendations of the Dentistry Sectional Committee (MGP 47) and approval of the Medical Instruments, General and Production Engineering Division Council. This Standard was first published in 1973 and was based substantially in agreement with lSO/R 1567: 1970. It was first revised in 1986 to align it with ISO 1567:1981 `Denture base polymers'. Its second revision has been undertaken to incorporate the modifications effected in the third addition of ISO 1567 brought out in 1999. In this revision modifications have been made for types and classes of denture base polymers, requirements and tests. Specific qualitative and quantitative requirements for freedom from biological hazard are not included in this standard, but it recommended that, in assessing possible biological or toxicological hazards, reference should be made to IS 12572 (Part 1): 1994 `Biological evaluation of medical devices -- Part 1 : Guidance on selection of tests (first revision) and IS 12572 (Part 10) : 1988 `Guide for evaluation of medical devices for biological hazards -- Part 10: Methods of biological testing and evaluation of dental materials'. The text of the ISO Standard has been approved as suitable for publication as an Indian Standard without deviations. Certain conventions are, however, not identical to those used in Indian Standards. Attention is particularly drawn to the following: a) Wherever the words `International be read as `Indian Standard'. Standard' appear referring to this standard, they should b) Comma (,) has been used as a decimal marker while"in Indian Standards, the current practice is to use a point (.) as the decimal marker. No. 1 to the above International Standard has been given at the end of this Standard. Amendment In the adopted standard, reference appears to certain International Standards for which Indian Standards also exist. The corresponding Indian Standards which are to be substituted in their places are listed below along with their degree of equivalence for the editions indicated: International Standard Corresponding Indian Standard Degree of Equivalence Identical ISO 1942-2 : 1989 Dental vocabulary -- Part 2 : Dental materials ISO 1942-5 : 1989 Dental vocabulary -- Part 5 : Terms associated with testing ISO 7491:1985 Dental materials -- Determination of colour stability of dental polymeric materials IS 7348 (Part 2): 2003 Dental vocabulary: Part 2 Dental materials (first revision) IS 7348 (Part 5) :1994 Dental vocabulary: Part 5 Terms associated with testing do IS 12181 :1987 Determination of colour stability of dental polymeric materials do (Continued on third coverj IS 6887:2005 ISO 1567:1999 Indian Standard DENTISTRY -- DENTURE BASE POLYMERS ( Second Revision) 1 Scope 1.1 This International Standard classifies denture base polymers and copolymers and specifies their requirements. It also specifies the test methods to be used in determining compliance with these requirements. It further specifies requirements with respect to packaging and marking the products and to the instructions to be supplied for use of these materials. 1.2 Although this International Standard does not require manufacturers to declare details of the composition, attention is drawn to the fact that some national or international authorities require such details to be provided. 1.3 a) b) c) d) e) f) 9) h) i) j) This International Poly(acrylic Standard applies to denture base polymers such as those listed below. acid esters); acrylic acid esters); poly(substituted poly(vinyi esters); polystyrene; rubber-modified polycarbonates; polysulfones; poly(dimethacrylic polyacetals copolymers acid esters); poly(methacrylic acid esters); (polyoxymethylene); or mixtures of the polymers listed in a) through i). 2 Normative references The folIowing standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. AH standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 463: --1 ), Geometrical product specifications Design and metrological requirements. ISO 1942-1:1989, (GPS) -- Dimensional measuring hstruments: Dial gauges -- Dents/ vocabulary -- Part 7: General and clinical terms. 1, To be published. (Revision of ISO 463:1 988) IS 6887:2005 ISO 1567:1999 ISO 1942-2:1989, ISO 1942-5:1989, ISO 3336:1993, ISO 3696:1987, ISO 7491:1985, ISO 8601:1988, times. Dental vocabuiaty -- Part 2: Dental materials. Dental vocabulary -- Pari 5: Terms associated Dentistry -- Synthetic po/yrner teeth. Water for ana/ytica/ /aboratory use -- Specification Dental materials -- Determination Data e/ements and interchange and test methods. with testing. of colour stability of dental polymeric materials. formats -- Information interchange -- Representation of dates and 3 Definitions For the purposes of this International Standard, the following definitions apply. 3.1 autopolymerizable polymers products having polymerization initiated by chemical means and not requiring application above 65 "C to complete the process of verifiable temperatures 3.2 capsulated material material consisting of two or more components supplied in a container which keeps them separated they are mixed together and dispensed for use directly from the container 3.3 denture artificial substitute function until the time for missing natural teeth and adjacent tissues, to include also any additions needed for optimum 3.4 denture base that part of a denture which rests on soft tissue foundations 3.5 heat-polymerizable polymer product requiring application of verifiable temperatures and to which teeth are added above 65 `C to complete polymerization 3.6 immediate container container which is in direct contact with the denture base materials 3.7 liquid monomeric fluid to be mixed with polymeric forming denture bases particles to form a mouldable dough or fluid resin mixture used for 3.8 outer packaging Iabelled container or wrapping within which other containers 3.9 packing (of a denture) technique) are packed the act of filling a denture base mould with a material (using a compression, pour or injection to form a denture base 2 . IS 6887:2005 1S0 1567:1999 3.10 initial packing time time after mixing, or other preparation, 3.11 final packing time the last time, after reaching consistency 3.12 processing procedure of preparing a solid denture base polymer plate and/or specimen by polymerization 3.13 thermoplastic, adj. characteristic of a hard polymeric at which a denture base material mixture first reaches packing consistence the initial packing time, at which a denture base material mixture retains packing or injection moulding material that allows it to be softened by application of heat to make it mouldable, and then return to the hardened state upon cooling 3.14 translucency capacity of a body of material to allow the passage of light, yet diffusing the light so as not to render objects lying beyond the body clearly visible 4 Classification Denture base polymers Classes: Type 1: Class 1: Class 2: Type 2: Class 1: Class 2: Type 3: Type 4: Type 5: covered by this International Standard are categorized into the following Types and Heat-polymerizable Powder and liquid Plastic cake Autopolymerizable Powder and liquid polymers polymers Powder and liquid pour-type resins Thermoplastic Light-activated Microwave blank or powder materials cured materials 5 Requirements 5.1 5.1.1 5.1.1.1 Unpolymerized material Liquid component General material compatible with the powder. The liquid shall consist essentially of monomeric IS 6887:2005 ISO 1567:1999 5.1.1.2 Homogeneity (8.1). The liquid shall be free of deposit or sediment that can be observed by visual inspection 5.1.2 Solid components components shall be free of extraneous The solid or semisolid (8.1). 5.1.3 material that can be observed by visual inspection Packing plasticity When Type 1 Class 1, Type 1 Class 2, Type 2 Class 1, Type 2 Class 2, Type 4 and Type 5 materials are tested in accordance with 8.2, at the initial packing time recommended by the manufacturer, they shall be capable of being intruded into at least two holes in the die (see figure 1) to a depth of not less than 0,5 mm (8.2.3.1.1). Type 1 Class 1, Type 1 Class 2, Type 4 and Type 5 materials shall also meet the requirements when tested at the final packing time (8.2.3.1 .2) 5.2 Polymerized material 5.2.1 Biocompatibility See the Introduction 5.2.2 Surface for guidance on biocompatibility characteristics When processed in the manner and against materials recommended by the manufacturer, denture base specimens prepared in accordance with 8.4.3, 8.7.2.2 and 8.8.3 should have a smooth, hard and glossy surface. The specimens for colour stability, the specimens for residual methyl methacrylate monomer sorption and volubility testing shall retain their form without visible distortion after processing. When polished (8.1). in accordance with 8.5.1.3, the specimen and the specimens for plates shall present a smooth surface with a high gloss When prepared in accordance with the manufacturer's instructions, all types of denture produce a test specimen plate (8.5.1) with defined edges after deflasking (see figure 3). 5.2.3 Colour base polymers shall A specimens strip shall show no more than a slight difference when compared with the corresponding shade guide, when tested in accordance with 8.3 and inspected in accordance with 8.1. The manufacturer shall provide a shade guide on request. shall be translucent (5.2.5 and 8.5.2) and evenly pigmented shade of the Coloured denture base polymers applicable, evenly fibred. and/or, where Clear denture base polymers shall be clear and colorless. 5.2.4 Colour stability with 8.1, test specimens shall not show more than When tested in accordance with 8.4 and inspected in accordance a slight change in colour, perceptible with difficulty. 5.2.5 Translucency When tested in accordance with 8.5.2.3 the shadow of the illuminated side of the test specimen plate. opaque disc shall be visible from the opposite 4 IS 6887:2005 ISO 1567:1999 5.2.6 Freedom from porosity with 8.5.3.3, specimens strips shall not show voids (8.1) that can be observed by When prepared in accordance visual inspection. 5.2.7 Flexural strength When determined in accordance with 8.5.3.5, the flexural strength shall be not less than 65 MPa for Type 1, Type 3, Type 4 and Type 5 polymers and not less than 60 MPa for Type 2 polymers when tested in water at (37 * 1) "C (see table 1). 5.2.8 Flexural modulus When determined in accordance with 8.5.3.5, the flexural modulus of the processed polymer shall be at least 2000 MPa for Type 1, Type 3, Type 4 and Type 5 polymers and at least 1500 MPa for Type 2 ~olymers when tested in water at (37 + 1) `C (see table 1). 5.2.9 Bonding to synthetic polymer teeth requirements. with Denture base polymers intended for use with synthetic polymer teeth shall meet one of the following a) The polymer shall, when tested in accordance the bonding requirements of ISO 3336. with 8.6, be capable of bonding to polymer teeth complying b) If there are problems of achieving bonding, the outer packages and containers shall contain information special treatments necessary to achieve bonding and/or indicate that further information is provided manufacturer's instructions [8.6.3, 9.2.1 k), 9.2.2 k), and 9.3 h)]. about in the 5.2.10 Residual methyl methacrylate monomer with 8.7, the following shall apply (see table 1). is 2,2 ?'. When prepared and tested in accordance The upper limit (maximum) for residual methyl methacrylate Type 1, Type 3, Type 4 and Type 5. The upper limit (maximum) Type 2. for residual methyl methacrylate mass fraction for denture base polymers of is 4,57. mass fraction for denture base polymers of If lower percentages of residual methyl methacfylate monomer are claimed by the manufacturer, not be more than 0,2 ?4. higher than that stated by the manufacturer. the content shall 5.2.11 Sorption shall When the processed polymer is tested in accordance with 8.8, the increase in volumic mass (water sorption) not exceed 32 pg/mm3 for Type 1, Type 2, Type 3, Type 4 or Type 5 polymers (see table 1). 5.2.12 Volubility polymer is tested in accordance with 8.8, the loss in volumic mass (soluble matter) shall not and shall not exceed 8,0 pg/mm3 for Type 2 When the processed exceed 1,6 pg/mm3 for Type 1, Type 3, Type 4 or Type 5 polymers, polymers (see table 1). 5 IS 6887:2005 ISO 1567:1999 Table 1 -- Summary of the limits for requirements Requirement Flexural strength [MPa] min. Type 1,3,4,5 Type 2 65 60 Flexural modulus [MPa] min. described in 5.2.7,5.2.8,5.2.10,5.2.1 Sorption 1 and 5.2.12 Volubility Residual methyl methacrylate monomer Percent mass fraction max. [pdmm~ max. [wimrn'1 max. 2000 1500 2,2 4,5 32 32 1,6 8,0 6 Sampling The test sample shall consist of a retail package or packages, containing sufficient material to carry out the specified tests, plus an allowance for any necessary repetition of the tests. If more than one package is required, all material shall be of the same batch. 7 7.1 Preparation Laboratory of test specimens environment instructions, the test specimens shall Unless otherwise specified in this International Standard or the manufacturer's be prepared and tested at (23 *2) "C and (50* 10) % relative humidity. 7.2 Procedures Unless otherwise specified in this International Standard, the materials used for making the specimens shall be prepared, manipulated and processed using the equipment and procedures recommended in the manufacturer's instructions (9.3) A separate ingredients. mix shall be made for each specimen prepared from a material requiring mixture of two or more 7.3 Special equipment a material shall be made available by the specimens, and submit them to the test Any special equipment specified by the manufacturer for processing manufacturer (or the manufacturer may prepare injection-moulded laboratory). 8 Test methods 8.1 Inspection for compliance determination Observe the test samples by visual inspection to determine compliance with the requirements laid down in 5.1.1.2, 5.1.2, 5.2.2, 5.2.3, 5.2.4, 5.2.5, 5.2.6 and clause 9. [Inspect for colour (5.2.3) and colour stability (5.2.4) in accordance with ISO 7491]. 8.2 8.2.1 Packing plasticity Apparatus brass die, having the dimensions shown in figure 1, with perforations having a diameter of 8.2.1.1 Perforated (0,75 * 0,05) mm. 6 IS 6887:2005 ISO 1567:1999 Dimensions in millimetres 50 t -1 A-A NOTE Dimensional tolerances notspecified shall be*l Figure 1 -- Perforated mm brass die for packing plasticity test (see 8.2) 8.2.1.2 8.2.1.3 8.2.1.4 Glass plate, (60 * 5) mm x (60* Weight, 5) mm x (5 f 1)mm. 1) N. 50 mm by 50 mm. " capable of exerting a force of (50* or polyester Polyethylene film, 0,035 mm to 0,050 mm thick and approximately 8.2.1.5 Dial gauge, complying with ISO 463, or linear gauge accurate to 0,01 mm, @quipped with a probe capable of entering holes in the brass die for measuring depth of penetration of the material into "the"die. 8.2.2 Test conditions at conditions specified in 7.1, except The perforated brass die (8.2.1.1 ) and glass plate (8.2.1.2) shall be maintained where otherwise specified by the manufacturer. 8.2.3 8.2.3.1 8.2.3.1.1 Procedure For Type 1 Class 1, Type 1 Class 2, Type 4 and Type 5 Initial packing time Prepare a sample of the material having a mass of 16 g to 20 g. Immediately prior to the manufacturer's recommended initial packing time [9.3 e)], shape one-half of the sample into a cake approximately 5 mm thick, 7 IS 6887:2005 ISO 1567: 1999 place it on the upper surface of the brass die (8.2.1.1) and cover it with a plastic sheet (8.2.1.4). At the recommended initial packing time, place the glass plate (8.2.1.2) and the weight (8.2.1.3) on the plastic-covered resin cake. After 10 min * 30s, remove the weight. When the material is firm, introduce the measuring instrument probe into each hole from the other side of the brass die, to contact the penetrating material to determine the depth in the hole not penetrated. Calculate the depth of penetration for each hole according to the following formula: DP=d­d' where DP d d' 8.2.3.1.2 is the depth of penetration, in millimetres; k the thickness of the brass die, in millimetres; k the the depth not penetrated, Final packing time by the manufacturer, shape the second half of the in millimetres. Immediately before the final packing time [9.3 e)] recommended sample into a cake and test this portion according to 8.2.3.1.1. 8.2.3.2 For Type 2, Class 1 Prepare a sample having a mass 8 g to 10 g. Shape this increment and test it according to the procedure in 8.2.3.1.1 8.2.3.3 For Type 2, Class 2 described Prepare a sample having a mass 8 g to 10 g. Introduce this increment onto the top surface of the brass die at the time recommended by the manufacturer [9.3d)] for pouring the fluid mix into the mould. Determine the depth of penetration values according to the procedure in 8.2.3.1.1 8.2.4 Pass/fail determinations specimens. If the second If the first specimen fails to comply with the requirement stated in 5.1.3, test two additional and third specimens comply with the requirement, the product passes. 8.2.5 Expression of results Report the number of holes penetrated material passes or fails. to a depth of not less than 0,5 mm by each specimen, and whether the 8.3 Colour with 8.5.3.3, and inspected in accordance with 8.1, with the Compare a specimen strip prepared in accordance shade guide for compliance with 5.2.3. 8.4 Colour stability 8.4.1 8.4.1.1 8.4.1.2 8.4.2 Materials Sheet of polyester film, having a thickness of (50* Aluminium Apparatus having the dimensions shown in foil. 25) pm, to cover the steel mould (8.4.2.1). 8.4.2.1 Stainless steel mould and cover (Type 1 and Type 2 materials), figure 2, mounted in gypsum in separate halves of a denture flask. 8 IS 6887:2005 ISO 1567:1999 Dimensions in millimetres 072tl t i 080il a m 7! m I I I t 2 Key 1 Mouid depth to form specimen 0,5+ 0,05 2 Mould 3 Cover NOTE Dimensional tolerances not specified shall be + 0,2 mm. 3 Figure 2 -- Stainless steel mould and cover for colour stability, sorption and volubility (see 8.4 and 8.8) 8.4.2.2 Moulds and/or equipment (Type 2 Class 2, Type 3, Type 4, Type 5 and capsulated recommended by the manufacturer to produce specimens with the dimensions specified in 8.4.3. 8.4.2.3 8.4.2.4 8.4.2.5 8.4.2.6 8.4.2.7 8.4.3 8.4.3,1 Hydraulic or hand press and clamp, where applicable. materials) Water bath, capable of maintaining constant temperatures, where applicable. Oven, capable of being maintained Micrometer at (37 * 1) `C. or dial calliper, accurate to 0,01 mm and fitted with parallel anvils. see 3.1.1 and 3.1.3 of ISO 7491:1985. Radiation source and test chamber, Preparation of test specimens Type 1 and Type 2 materials Make two specimens from separate mixes. Mix the resin and pack the mixture into the mould (8.4.2.1) with the polyester film (8.4.1.1 ) against the steel cover of the mould. Process the mixture in accordance with the manufacturer's instructions, but retain the polyester film during the processing cycle. 9 IS ISO 6887:2005 1567:1999 8.4.3.2 Type 2 Class 2, Type 3, Type 4, Type 5 and capsulated materials Prepare the specimens as described by the manufacturer. Check with a micrometer or dial calliper (8.4.2.6) to ensure that each specimen has a diameter of (50 * 1) mm and a thickness of (0,5 * 0,1) mm and that the top and bottom surfaces are flat. 8.4.4 Procedure Store the two specimens in the oven (8.4.2.5) for 24 h * 30 min. Then store one specimen in the dark in laboratory environment (7.1 ) until the colour comparison test is made. Cover half of the second specimen with aluminium foil (8.4.1 .2) and transfer it to the radiation source and test chamber (8.4.2.7). The specimen shall be immersed in water at (37 * 5) "C when exposed to the radiation for 24 h *30 min in accordance with ISO 7491. After exposure, remove the aluminium foil before colour comparison of the specimens including the unexposed specimen. The colour International comparison shall be carried out in accordance with the requirements specified in 5.2.4 of this Standard and in accordance with the procedure for colour comparison laid down in ISO 7491. specimen in laboratory environment (7.1) for 6 d * 2 h until the colour For Type 4 materials, store the exposed comparison test is made. 8.5 8.5.1 8.5.1.1 Polishability, Polishability Apparatus translucency, freedom from porosity, flexural strength and flexural modulus 8.5.1.1.1 Denture flask, capable of accommodating the test specimen plate so that the corners are not less than 5 mm from the walls of the flask. 8.5.1.1.2 Model of the specimen plate, in metal or polymer (see figure 3). Dimensions in millimetres NOTE Dimensional tolerances shall be* 1 mm. Figure 3 -- Model of the specimen plate (see 8.5) 8.5.1.1.3 8.5.1.1.4 Equipment for processing Standard metallographic the resin, including gypsum or hydrocolloid [9.3 f)]. 30 pm. grinding paper, with a grain size of approximately 10 IS 6887:2005 "ISO 1567:1999 NOTE Grinding paper with a 500 FEPA (Federation europenne des produits abrasifs: European Federation for Abrasive Products) standard number is recommended; however any other paper meeting the same requirements is suitable. 8.5.1 .1.5 8.5.1 .1.6 Wet pumice, having a grain size of approximately 10 pm to 20 pm. Polishing compound. 8.5.1 .1.7 Muslin wheel, with 16 to 36 ply, having a diameter of 70 mm to 95 mm and at least 10 mm between the outer diameter and the stitching or other reinforcement. 8.5.1 .1.8 8.5.1.2 Unstitched Preparation muslin wheel, with 16 to 36 ply, having a diameter of 70 mm to 95 mm. of the mould For Type 1 and Type 2 Class 1 polymers, invest the model of the specimen plate (8.5.1.1.2) in the denture flask (8.5.1 .1.1 ) in accordance with the manufacturer's instruction. Prepare the mould for Type 2 Class 2 ,Type 3, Type 4, Type 5 and capsulated materials in accordance with the manufacturer's instructions. 8.5.1.3 Procedure Form and process according to the manufacturer's instruction two specimen plates each from a separate mix. Use the material, the equipment (8.5.1. 1) and the mould (8.5.1.2). Grind and polish surfaces of the specimen plates for not longer than 1 min with pumice (8.5.1.1 .5) and with a wet muslin wheel (8.5.1.1 .7) at a circumferential speed of (650 * 350) m/min. (A wheel with a diameter of 70 mm rotating at 1500 rein-l will have a circumferential speed of 329 m/min and a 100 mm diameter wheel rotating at 3500 rein-l will have a circumferential speed of 1100 m/min). Thereafter polish with an unstitched muslin wheel (8.5.1.1.8) with a polishing compound (8.5.1.1 .6). After polishing and cleaning, examine the polished surfaces for compliance with 5.2.2. 8.5.1.4 Pass/fail determination If both specimen plates comply with 5.2.2, the material passes. If both specimen plates fail to comply with 5.2.2, the material fails. If only one of the specimen plates complies, prepare and evaluate three new plates. The material passes only if all three new plates comply. 8.5.1.5 Expression of results Report the number of specimen plates evaluated, the number complying and whether the material passes. 8.5.2 8.5.2,1 8.5.2.1.1 8.5.2.2 8.5.2.2.1 8.5.2.2.2 8.5.2.3 Translucency Materials Two specimen Apparatus Opaque disc, of diameter (10* Frosted 40 W electrical Procedure 1) mm and thickness (2* 1) mm. plates, prepared and tested according to 8.5.1. light bulb. Examine each of the two specimen plates separately. Position the polished specimen plate approximately 500 mm from the light bulb (8.5.2.2.2) with the opaque disc (8.5.2.2.1 ) centred on the surface nearest the light bulb. Darken the room. View the specimen plate from the side opposite the disc location to determine whether the material complies with 5.2.5. 11 IS 6887:2005 ISO 1567:1999 8.5.2.4 Pass/fail determination If both specimen plates comply with 5.2.5, the material passes. If both specimen plates fail, the material fails. If only one of the specimen plates passes, prepare and evaluate three new plates. The material passes only if all three new plates comply. 8.5.2.5 Expression of results Report the number of specimen plates evaluated, the number complying and whether the material passes. 8.5.3 Freedom from porosity, flexural strength and flexurai modulus 8.5.3.1 8.5.3.1.1 8.5.3.2 8.5.3.2.1 Materials Two specimen plates, prepared and tested according to 8.5.1 and 8.5.2. Apparatus Sawing machine, or other cutting device for sectioning the specimen plates. 8.5.3.2.2 Milling machine, or other instrumentation for air or water cooled cutting so as not to generate temperatures above 30 "C during shaping of the specimens. (A machine with a milling head and a sharp carbide edge, is suitable.) 8.5.3.2.3 Standard metallographic grinding and 14 pm (1200 FEPA). See note in 8.5.1.1.4. 8.5.3.2.4 8.5.3.2.5 Micrometer, papers, having a grain size of approximately 30pm (500 FEPA) and/or dial calliper accurate to 0,01 mm and fitted with parallel anvils. Container of water, for storing the specimen strips at (37 * 1) "C for pre-test conditioning. Testing machine, calibrated to provide for a constant crosshead speed of (5 i 1) mm/min and equipped 8.5.3.2.6 with instrumentation for measuring the deflection of the specimen to within' 0,025 mm. Any load exerted by the deflection instrument shall be accounted for when calibrating the machine. 8.5.3.2.7 Flexural test rig, consisting of a central loading plunger and two polished cylindrical supports, 3,2 mm in diameter and at least 10,5 mm long. The supports shall be parallel to within 0,1 mm and perpendicular to the longitudinal centreline. The distance between centres of the supports shall be (50 * 0,1) mm, and the loading plunger shall be midway between the supports to within 0,1 mm. Means to prevent misalignment of the specimen shall be included in !he design. 8.5.3.2.8 8.5.3.3 Water bath, for maintaining the specimens wet and at a temperature of (37* Procedure 1) `C, during testing, Prepare six specimen strips. Cut each plate lengthways into three equal strips, 64 mm long, (10,0 * 0,2) mm wide and (3,3 & 0,2) mm in height. Machine the strips in a milling machine (8.5.3.2.2) on the edges and equally from both moulded surfaces so that the dimensions remain slightly oversized. Take care to avoid overheating the specimen. Wet-grind all faces and edges smooth and flat with the metallographic grinding papers (8.5.3.2.3) to the required width and height. Three measurements of the specimen height shall be made along the long axis with an accuracy of & 0,01 mm. The deviation between the three measurements along the long axis shall be not more than * 0,02 mm. The specimen shall be flat and have an even height. 8.5.3.4 8.5.3.4.1 Freedom from porosity Pass/fail determination with 8.5.3.3 and examined for compliance witA 5.2.6. Six test specimen strips shall be prepared in accordance 12 IS ISO 6887:2005 1567':1999 The material passes only if at least five out of six specimen strips comply with the requirement 8.5.3.4.2 Expression of results and whether the material passes. in 5.2.6. Report the number of specimen strips complying 8.5.3.5 8.5.3.5.1 Flexural strength and flexural modulus Procedure according to 8.5.3.3 and complying with 5.2.6, in water at a flexural t&ting. Take a specimen s~rip from water storage and the supports of the flexural test rig (8.5.3.2.7) immersed in the to equilibrium with the water bath temperature. speed of (5 * 1) mrn/min Store the five or six sDecimen strbs, l)reDared temperature of (37 * 1)' "C for (50 ~ 2) h p'rior to immediately lay the flat surface symmetrically on water bath (8.5.3.2.8). Allow the specimen to come Increase the force on the loading plunger from zero, uniformly, using a constant crosshead until the specimen breaks. 8.5.3.5.2 8.5.3 .5.2.1 Calculation and expression of results Flexural strength from the following equation: Calculate the flexural strength, o, in megapascals ~ = 3F1 2bh2 where F 1 b h is the maximum load, in newtons, exerted on the specimen; is the distance, in millimetres, k the width, in millimetres, is the height, in millimetres, Flexural modulus from the following equation: between the supports, accurate to* 0,01 mm; prior to water storage; prior to water storage. of the specimen measured immediately of the specimen measured immediately 8.5.3 .5.2.2 Calculate the flexural modulus E, in megapascals, where F1 is the load, in newtons, at a convenient point in the straight-line portion of the trace; NOTE For greater accuracy, the straight line may be extended. d 1, b and h 8.5.3 .5.2.3 is the deflection, in millimetres, at load F1; are as defined in 8.5.3.5.2.1. of flexural strength Pass/fail determination If at least four of the results out of five specimens are not less than 65 MPa for Type 1, Type 3, Type 4 and Type 5 polymers and not less than 60 MPa for Type 2 polymers, the material is deemed to have complied with the requirements of 5.2.7. 13 IS 6887:2005 ISO 1567:1999 If at least three of the results are less than 65 MPa for Type 1, Type 3, Type 4 and Type 5 polymers and less than 60 MPa for Type 2 polymers, the material is deemed to have failed absolutely. If two of the results are less than 65 MPa for Type 1, Type 3, Type 4 and Type 5 polymers and 60 MPa for Type 2 polymers, repeat the whole test but on this occasion prepare six specimen strips. If at least five of the results are not less than 65 MPa for Type 1, Type 3, Type 4 and Type 5 polymers and not less than 60 MPa for Type 2 polymers on the second occasion, the material is deemed to have complied with the requirements of 5.2.7. 8.5.3 .5.2.4 Pass/fail determination of flexural modulus If at least four of the results passed the requirements of 5.2.7 on the first occasion, calculate the flexural modulus according to 8.5.3 .5.2.2 for each of the five specimens. If a second series was tested, calculate the flexural modulus for five of the six specimens from this series only. If at least four of the results are not less than 2000 MPa for Type 1, Type 3, Type 4 and Type 5 polymers and not less than 1500 MPa for Type 2 polymers the material is deemed to have complied with the requirements of 5.2.8. If at least three of the results are less than 2000 MPa for Type 1, Type 3, Type 4 and Type 5 polymers than 1500 MPa for Type 2 polymers, the material is deemed to have failed absolutely. and less If two of the results are less than 2000 MPa for Type 1, Type 3, Type 4 and Type 5 polymers and less than 1500 MPa for Type 2 polymers, repeat the whole test, but on this occasion prepare six specimen strips. In this series, at least five results for both flexural strength and flexural modulus shall comdv . . with the requirements of 5.2.7 and 5.2.8. 8.5.3 .5.2.5 Expression of results modulus with the Report the number of specimen strips evaluated, all results for flexural strength and flexural number of strips complying with the 5.2.7 and 5.2.8, and whether the material passes. 8.6 8.6.1 Bonding Materials to synthetic polymer teeth 8.6.1.1 8.6.1.2 8.6.2 Maxillary anterior synthetic Dental mounting wax. Apparatus polymer teeth complying with ISO 3336. 8.6.2.1 Metal form, of the design illustrated in figure 3 a) of ISO 3336:1993, wide by 1,5 mm deep for use in mounting the teeth. which incorporates a trough 5 mm Normal dental laboratory 8.6.2.2 hydrocolloid [9.3 f)]. 8.6.2.3 8.6.3 Tensile testing apparatus Procedure apparatus for denture flasking and processing, including gypsum or with specially designed grips illustrated in figure3c)ofISO3336:1993. Grind the ridge lap of a set of six maxillary anterior teeth (8.6.1 .1). Mount these teeth on a metal form (8.6.2.1) with wax (8.6.1 .2), as illustrated in figure 3 a) of IS(3 3336:1993, so that about one-half of the lingual surface of the incisal portion of the tooth projects beyond the metal form. 14 IS 6887:2005 ISO 1567:1999 Using a denture flask (8.6.2.2), set the mounted teeth in dental gypsum [figure 3 b) of ISO 3336:1993]. Remove the metal form and then flush the wax from the teeth with boiling tap-water containing a detergent until all wax has been removed, followed by rinsing several times with boiling tap-water. Prepare and process the denture base polymer to the teeth according to the manufacturer's instructions (9.3) after proper plasticity has been reached. Test the denture base-mounted teeth in the tensile testing apparatus (8.6.2.3) designed to permit a direct pull on the incisal part of the lingual surface in a labial direction at a consistent height above the acrylic bar [figure 3 c) of ISO 3336:1993]. Use equipment which does not permit lateral deflection or change of position. Load each tooth, as illustrated in figure 3 c) of ISO 3336:1993, 10 mm/min until fracture occurs. 8.6.4 Pass/fail determination at a displacement rate in the range 0,5 mrn/min t.o The bond passes the test if the fracture path does not occur cleanly along the tooth surface. Thus, tooth remnants shall remain bonded to the denture base polymer and/or denture base polymer shall remain firmly bonded to the detached tooth or the adhesive shall remain firmly bonded to both detached tooth and denture base. NOTE Only pure adhesive interracial fracture indicates a failure to meet the requirement. Cohesive fracture in either the tooth, the denture base polymer or an adhesive, is necessary for a satisfactory bond. If at least five maxillary requirement of 5.2.9. anterior teeth pass the test, the denture base polymer is deemed to comply with the If only three comply, the denture base polymer fails. If only four comply, prepare an additional denture base polymer with six maxillary anterior teeth from one set. If at least five maxillary anterior teeth pass this second test, the denture base polymer is deemed to comply with the requirement. 8.6.5 Expression of results Report the number of teeth for which the bond passes the test. 8.7 8.7.1 Residual methyl methacrylate monomer Principle (MMA) monomer from polymerized denture base materials is carried Solvent extraction of the methyl methacrylate out, followed by chromatographic analyses. A gas chromatographic (HPLC) method (annex A) or any (GC) method, high performance liquid chromatography other chromatographic method which gives the same results as the methods of this International Standard can be used. This shall be verified International Standard. by proficiency testing based on the chromatographic methods described in this 8.7.2 8.7.2.1 Preparation Apparatus of test specimen discs 8.7.2.1.1 Circular stainless steel mould (Type 1 and Type 2), with a diameter of 50 mm and a depth of (3,0 * 0,1) mm with a flat cover. A similar mould (less deep) is shown in figure 2. The mould shall be mounted in 9YPsum in separate halves of a denture flask. 8.7.2.1.2 Moulds ancf/or equipment (Type 2 Class 2, Type 3, Type 4, Type 5 and capsulated recommended by the manufacturer to produce specimens with the dimensions specified in 8.7.2.1.1. 8.7.2.1.3 Standard metallographic grinding 15 pm (1200 FEPA). See note of 8.5.1.1.4. papers, with a grain size of approximately 30pm materials) (500 FE PA) and . 15 IS 6887:2005 ISO 1567:1999 8.7.2.2 Procedure Prepare three specimens from three separate mixes as described in 8.4.3, except that the mould shall have the dimensions given in 8,7.2. 1.1. Keep the specimens in the dark at laboratory environment (7.1) for (24 * 5) h prior to grinding. Use the metallographic grinding papers (8.7.2.1.3) in turn, to wet-grind material equally from both sides of the specimen disc, until a thickness of (2,0 * 0,1) mm is obtained. Grind the periphe~ of the specimens against the 15 pm grain metal lographic grinding paper until the entire periphery is abraded and smooth. Avoid frictional heat which can cause loss of monomer or depolymerization. Examine the specimens visually without magnification. If the specimen demonstrates minimal porosity, then three samples can be obtained from it. NOTE If the specimens are stored in the refrigeratorthe monomer content remains constant for several days. If the specimens are stored in the freezer (below -18 "C) the monomer content remains constant for several months. Store the ground specimens in the dark at laboratory environment 8.7.3 8.7.3.1 8.7.3.1.1 8.7.3.1.2 8.7.3.1.3 Extraction Reagents Hydroquinone (HQ). of monomer for (24* 1) h prior to extraction of monomer. Acetone, of analytical or HPLC grade. Methanol (CH30H), of analytical or HPLC grade. 8.7.3.1.4 Internal Standard (1.S.) mpentanol, of analytical grade, or any other suitable 1.S. (e.g. 1-butanol) whose peak does not interfere with any other peak in the sample solution. 8.7.3.2 Apparatus Ordinary laboratory apparatus and 8.7.3.2.1 8.7.3.2.2 8.7.3.2.3 8.7.3.2.4 8.7.3.2.5 8.7.3.2.6 8.7.3.3 8.7.3.3.1 Magnetic stirring apparatus, Analytical One-mark with PTFE-coated magnetic stirring bar. balance, with an accuracy of 0,1 mg or better. volumetric glass flasks, of capacities 5 ml, 10 ml and 11. Glass centrifuge tubes. Volumetric Centrifuge, Preparation pipettes, of capacities 100 PI, 2 ml, 3 ml and 5 ml. capable of centrifugingat3000 of solutions gn mLs2. Acetone solution (A) into a 1 I one-mark volumetric glass flask (8.7.3.2.3). Add acetone Weigh approximately 0,02 g HQ (8.7.3.1.1) (8.7.3.1 .2) until the total volume is 11. 8.7.3.3.2 Methanol solution (B) Weigh approximately 0,02 g HQ (8.7.3.1.1.1) (8.7.3.1 .3) until the total volume is 11. 8.7.3.3.3 Methanol/acetone solution (C) into a 1 I one-mark volumetric glass flask (8.7.3.2.3). Add methanol Mix one volume part of solution A (8.7.3.3.1) and four volume parts of solution B (8.7.3.3.2). 16 IS 6887:2005 ISO 1567:1999 8.7.3.3.4 internal Standard (l. S.)solution the calibration curve, (8.7.3.2.3). Add the ensure that there is will be approximately acetone solution (A) In order to achieve an 1.S. peak which will represent a concentration located in the middle of weigh approximately 350 mg IS. (8.7.3.1 .4) into a 10 ml one-mark volumetric glass flask methanol solution (B) (8.7.3.3.2) until the total volume is 10 ml. The volume of 10 ml is to enough I.S. solution for additional analyses. The concentration of the I.S. in the final solution 3 % mass fraction of the quantity of the specimen pieces (e.g. 650 mg) treated with the (8.7.3.3.1) and the methanol solution (B) (8.7.3.3.2). 8.7.3.3.5 Sample solutions Analyse three sample solutions from each test specimen, i.e. a total of nine sample solutions. Break each specimen disc (8.7.2) into pieces small enough to pass through the neck of the one-mark 10 ml volumetric glass flasks (8.7.3.2.3). A sample size of approximately 650 mg is introduced into separate one-mark volumetric glass flasks. The mass is weighed out with an analytical balance (8.7.3.2.2) and recorded for each individual sample solution. q Add the acetone solution (A) (8.7.3.3.1 ) until the total volume is 10 ml and then introduce a clean PTFE coated magnetic stirring bar (8.7.3.2.1 ) to each one-mark volumetric glass flask. Ensure that the volumetric one-mark glass flasks are properly sealed and agitate the sample solutions by magnetic stirring for (72 *2) h at room temperature. To precipitate the dissolved polymer, use a separate volumetric pipette (8.7.3.2.5) to transfer a 2 ml aliquot of each previously prepared sample solution to each one-mark 10 ml volumetric flask. Then add 100 PI of the IS. solution (8.7.3.3.4) sample solutions to a total volume of 10 ml. to each flask. Add methanol solution (B) (8.7.3.3.2) to each of these Use separate volumetric pipettes (8.7.3.2.5) to transfer 5 ml of the polymer each of the 10 ml flasks to glass centrifugation tubes (8.7.3.2.4). Centrifuge the slurry at 3000 gn m/s2 for 15 min in a centrifuge (8.7.3.2.6). and monomer containing slurry from Use separate volumetric pipettes to transfer a 3 ml aliquot of each centrifuged solution to separate glass tubes. Determine that there is no remaining polymer in the solution by adding additional amounts of methanol to an aliquot of the remaining centrifugate in a test tube. The centrifugate shall appear clear when a beam of light is directed vertically through the test tube containing the solution. This test shall be carried out in a dark room. If the solution does not appear clear, repeat the procedure described above using a larger amount of the methanol solution (B). Record the volume of the methanol solution (B) necessary to complete precipitation of polymer. When the solution appears clear, determine the residual monomer content by means of the GC method, HPLC method (annex A) or another equivalent chromatographic method (8.7.1). 8.7.4 8.7.4.1 8.7.4.1.1 8.7.4.2 Gas chromatography Reagent Methyl methacrylate Apparatus (MMA), GC-purity >99 ?!.. 8.7.4.2.1 Gas chromatography with splitkplitless injection port for liquid samples (split mode 1:10 recommended) flame ionization detector and recording system. 8.7.4.2.2 Microsyringe, capacity 0,1 PI to 5 PI. 17 IS 6887:2005 ISO 1567:1999 8.7.4.3 8.7.4.3.1 Procedure Preparation of calibration solutions for gas chromatography Make at least five standard solutions with concentrations of MMA between approximately 0,1 Y. mass fraction to approximately 6 `Y. mass fraction of the quantity of the specimen pieces. Prepare calibration solutions of MMA by weighing approximately 6 mg, 60 mg, 150 mg, 300 mg and 400 mg of MMA (8.7.4.1 .1) into separate one-mark volumetric glass flasks of capacity 5 ml (8.7.3.2.3). Add solution C (8.7.3.3.3) until the total volume is 5 ml. Transfer 100 PI of each calibration solution into separate 10 ml one-mark volumetric glass flasks together with 100 PI of the 1.S. solution (8.7.3.3.4); add solution C until the total volume is 10 ml. Record the mass of MMA for each micrograms per millilitre. individual calibration solution and calculate the final concentrations, in If the MMA content of the sample solutions graph, make additional calibration points. does not fit within the extreme MMA concentrations of the calibration 8.7.4.4 a) Gas chromatographic equipment, gases and operating conditions Column: stationary glycol; "fused silica capillary tube of length 30 m and internal diameter 0,25 mm is recommended; a phase of a polysiloxane derivative (e.g. polysiloxane with methyl and phenyl groups) or polyethylene b) c) d) e) f) 9) column conditioning: recommended 6 h to 10 h under gas flow and at elevated temperatures; 75 "C, isothermal; column temperature: 200 "c; 200 `c; injector temperature: detector temperature: carrier gas: helium for gas chromatography with a flowrate of approximately 1,3 ml/min; fuel gases: hydrogen and air for gas chromatography. 8.7.4.5 Gas chromatograms of sample and calibration solutions Depending on the sensitivity of the gas chromatography used, inject a suitable volume of sample solution (prepared according to 8.7.3.3.5) or the calibration solution (prepared according to 8.7.4.3.1). The injected volume is not critical for the calculation of results, but shall be identical for corresponding samples and calibration solutions. Operate the gas chromatography until all components are completely eluted. To ensure correct quantification of the MMA content in the sample solutions, good separq!ion be secured by using different column oven temperature profiles. of all substances shall 8.7.4.6 Evaluation of peaks of gas chromatogram The retention times of MMA and 1.S. shall be known, at least in relation to each other. The exact values vav according to the age of the column and other gas chromatographic parameters. The peak height or area of MMA and I.S. shall be determined by electronic registration and integration. 8.7.5 8.7.5.1 Calculation Calculation and expression of results graph of results from a calibration 18 IS 6887:2005 ISO 1567: 1999 8.7.5.1.1 Drawing of thecalibration graph Draw a calibration graph by plotting the ratios of the peak area (or height): %IMA `&s. where AMMA 4:s. 8.7.5.1.2 is the peak area (or height) of methyl methacrylate monomer in the calibration solution; solution. is the peak area (or height) of internal standard (e.g. n-pentanol) in the calibration Precision of measurements graph established by linear regression shall be not less than 0,990. The correlation coefficient of the calibration 8.7.5.1.3 Determination of the percentage of methyl methacrylate ratio: Determine the percentage AMMA `%s, where `MMA "$.s. of MMA using the corresponding is the peak area (or height) of methyl methacrylate in the sample solution; in the sample solution. is the peak area (or height) of internal standard (e.g. rt-pentanol) graph to determine the concentration, in micrograms Use the calibration sample solution. of MMA (CMMA) per millilitre of analysed Total qUantity Of MMA in the Sample SOhJtiOn,mMMA (pg), is calculated according to the equatiOn: a, For precipitation of dissolved polymer, methanol solution (B) is added to a 2 ml aliquot of the sample solution and 100 PI LS. solution in a volumetric closed glass flask until a total volume of 10 ml is achieved. If complete precipitation of polymer is not achieved with a 2:10 dilution, this factor shall be altered. The volume of the original sample solution was 10 ml. `MMA x 100 msAMpLE b) Residual monomer (% mass fraction)= where msAMPLE is the mass of sample, in micrograms. 8.7.5.2 Pass/fail determinations for at least seven of the sample solutions comply with the requirement stated in 5.2.10, the If results obtained material passes. If four or fewer of the sample solutions comply with the requirement stated in 5.2.10, the material fails, If only five or six comply, make new specimen discs and solutions and repeat the test. If at least eight of the second series of solutions comply with the requirement stated in 5.2.10, the material passes. 19 IS ISO 6887:2005 1567:1999 8.7.5.3 Expression of results Report the number of sample solutions evaluated, all results for residual monomer content and whether the material passes. 8.8 Water sorption and volubility 8.8.1 Materials 8.8.1.1 8.8.1.2 8.8.2 8.8.2.1 8.8.2.2 8.8.2.3 8.8.2.4 8.8.2.5 8.8.2.6 8.8.2.7 8.8.3 Silica gel, freshly dried for (300 * 10) minat(130 Water, complying with grade 2 of ISO 3696. Apparatus * 5) "C. Rack to keep the specimens parallel and separated. Two desiccators. Oven, maintained Polymer-coated Clean dry towel. Micrometer, accurate to 0,01 mm. at (37* 1) "C. tweezers. Dial gauge calliper or slide calliper, accurate to 0,01 mm. Preparation of test specimens Specimens 8.8.4 8.8.4.1 shall be prepared as described in 8.4.3, except that five specimens shall be prepared. Procedure Conditioned specimens Place the specimens in the rack (8.8.2.1) inside one of the desiccators (8.8.2.2) containing freshly dried silica gel (8.8.1.1 ). Store the desiccator in the oven (8.8.2.3) at (37 + 1) "C for (23* 1) h and then remove the desiccator from the oven. Transfer the specimens kept in the rack directly to the second desiccator which has beerl supplied with freshly dried silica gel. The second desiccator is kept at (23 * 2) `C. After (60 * 10) min in the second desiccator, the specimens are ready for weighing. Use an analytical balance (8.7.3.2.2) to weigh the specimen to an accuracy of 0,2 mg. Keep the desiccator sealed except for the shortest possible period required for removing and replacing specimens. After all the specimens have been weighed, replace the silica gel in the first desiccator with freshly dried gel and place the desiccator in the oven. Repeat the cycle described until a constant mass, ml, to be called the "conditioned mass", is reached, i.e. until the loss in mass of each specimen is not more than 0,2 mg between successive weighings. At this point calculate the volume V of each specimen, using the mean of three diameter measurements and the mean of five thickness measurements. The thickness measurements are taken in the centre and at four equally spaced locations around the circumference. 8.8.4.2 Wet specimens Immerse the conditioned specimens in water (8.8.1 .2) at (37 * 1) "C for 7 d * 2 h. After this time, remove the discs from the water with polymer-coated tweezers (8.8.2.4), wipe with a clean dry towel (8.8.2.5) until free from visible 20 IS 6887:2005 ISO 1567:1999 moisture, wave in the air for (15 t 1) s and weigh (60 * 10) s after removal from the water (with an accuracy 0,2 mg). Record this mass as mz. 8.8.4.3 Reconditioned specimens as described of After this weighing, recondition the specimens to constant mass in the desiccator the mass of the "reconditioned" specimens as ms. in 8.8.4.1. Record It is essential that the same conditions be applied as for the first drying process (8.8.4.1), using the same number of specimens and the freshly dried silica gel in the desiccators. 8.8.5 8.8.5.1 Calculation and expression of results Water sorption WSPfor each specimen, expressed in micrograms Per cubic millimetre Calculate the value for the water sorption, (lJ9/mm3) from the following equation: where m2 m3 v is the mass of the specimen, is the reconditioned in micrograms (pg), after immersion in water (8.8.4.2); mass of the specimen, in micrograms in cubic millimetres (pg) (8.8.4.3); is the volume of the specimen, (mms) (8.8.4.1). per cubic millimetre (pg/mm3). Round off the values calculated for water sorption to the nearest microgram 8.8.5.2 Water volubility Calculate the soluble matter per unit volume, WSI, leached out during immersion, millimetre (pg/mm3 ) for each specimen from the following equation: expressed in micrograms per cubic Wsl= where ml m3 ml ­ ms -- v is the "conditioned" mass of the specimen, in micrograms (pg) (see 8.8.4.1); and V are as given in 8.8.5.1. Round off the values calculated for water volubility to the nearest 0,1 pg/mm3. 8.8.5.3 Pass/fail determination of water sorption stated in 5.2.11, the material passes. stated in 5.2.11, the material is If at least four of the water sorption results comply with the requirement If at least three of the water sorption deemed to have failed absolutely. results do not comply with the requirement If only three of the water sorption results comply with the requirement stated in 5.2.11, prepare and test a series of six additional specimens. If at least five of the water sorption results of the second series comply with the requirement stated in 5.2.11, the material is deemed to have passed. 21 IS 6887:2005 ISO 1567: 1999 8.8.5.4 Pass/fail determination ofwatersolubility stated in 5.2.12, the material passes. stated in5.2.12, the materials is If at least four of the water volubility results comply with the requirements If at Ieasttwo of the water volubility deemed to have failed absolutely. results do not comply with the requirements If only three of the water volubility results comply with the requirements stated in 5.2.12, prepare and test a series of six additional specimens. If at least five of the water volubility results of the second series comply with the requirements stated in 5.2.12, the material is deemed to have passed. 8.8.5.5 Expression of results with the number of Report the number of specimens evaluated, all results for water sorption and water volubility specimens complying with the 5.2.11 and 5.2.12, and whether the material passes. 9 Requirements by manufacturer 9.1 Packaging for Iabelling, marking, packaging and instructions supplied The material shall be supplied in properly sealed containers made of materials which neither contaminate nor allow contamination of the contents. The containers shall be packaged so as to prevent damage or leakage during transit and storage. The liquid shall be contained in a dark-coloured bottle or opaque container. An outer package may be used to present one or more immediate containers for retail marketing. 9.2 Marking of outer packages and containers 9.2.1 Outer packages Each outer package shall be clearly marked with the following information: a) b) c) d) the trade or brand name of the material; manufacturer's name and address and/or agent in country of sale; given in clear language; year and month; the Type, Class and colour of the material and its application the term expiry date followed by a four-digit number indicating the applicable EXAMPLE: Expiry date 9607, where the first pair of digits represents the year 1996 and the second pair of digits represents the month July (ISO 8601). e) f) 9) h) i) recommended the specification cautionary cautionary conditions of storage; of the contents, including the number, mass and/or volume of each item; with regard to flammability and flashpoint of the liquid (when applicable); or irritating characteristics; present in the material and referred" to in product statements statements with regard to toxic, hazardous, identification of any pharmaceutically active ingredients information and instructions provided by the manufacturer manufacturer's batch reference: information j) k) where applicable, of any special treatment to achieve bonding to synthetic polymer teeth (5.2.9). 22 IS 6887:2005 ISO 1567:1999 9.2.2 All immediate containers All immediate containers shall be clearly marked with the following information: a) b) c) d) the trade or brand name of the material; manufacturer's name and address and/or agent in country of sale; given in clear language; year and month; the Type, Class and colour of material and its application the term expiry date followed by a four-digit number indicating the applicable EXAMPLE: Expiry date 9607, where the first pair of digits represents the year 1996 and the second pair of digits represents the month July (ISO 8601). e) f) 9) h) i) recommended specification conditions of storage; of the contents, including the number, mass and/or volume; and flashpoint of the liquid (if applicable); cautionary statements with regard to flammability cautionary statements with regard to toxic, hazardous, or irritating characteristics; identification of any pharmaceutically active ingredients information and instructions provided by the manufacture~ manufacturer's batch reference; information of any special treatment to achieve bonding to synthetic polymer teeth (5.2.9). materials present in the material and referred to in product j) k) 9.2.3 where applicable, Containers of powder, blank and plastics The colour shall be clearly marked on each container of powder. 9.2.4 Containers of liquid The flashpoint of the liquid shall be clearly marked on each container of liquid. 9.3 Manufacturer's instructions The instructions needed for safe and effective use of the material shall be included in each individual package. All processing methods described in the manufacturer's instructions shall result in a denture base polymer which fulfils the requirements laid down in this International Standard. As a minimum they shall include (as applicable) the following information: a) b) recommended storage conditions for unprocessed prolonged skin contact material; gel or liquid and against inhalation of the cautions against monome~ powder/liquid with the unpolymerized c) d) e) f) 9) ratio (mass per unit volume or mass fraction); and procedures to prepare the material for packing; initial packing time and final packing time; time, temperature time over which packing may be effectively conducted: equipment and material needed to prepare the mould (e.g. type of flask, gypsum, hydrocolloid); separation media; recommended 23 IS 6887:2005 ISO 1567:1999 h) i) j) k) 1) m) any special treatment temperature necessary to achieve bonding to synthetic polymer teeth; of the flask during packing; polymerization of the material; detailed procedure for activating and completing post-processing . maximum treatment of the processed material (cooling and storage after deflasking); residual monomer content (percent mass fraction) when tested according to 8.7; `Yo. curing cycle necessary to achieve a residual monomer content claimed to be less than 1 NOTE Special instructions may be necessary for the equipment and processing of Type 2 Class 2, Type 3, Type 4, Type 5 and capsulated material as indicated in 8.4.3 and 8.5.1.2. 24 IS 6887:2005 ISO 1567:1999 Annex A (normative) HPLC method for determination of MMA content NOTE see 8.7. Several items needed for the HPLC method are identical to some of those required for use in the GC method, A.1 Preparation of test specimens See 8.7.2. A.2 Extraction of monomer A.2.1 Reagents A.2.1.1 A.2.1.2 A.2.1.3 A.2.2 Reagents as described in 8.7.3.1. Tetrahydrofuran Water, complying Apparatus in 8.7.3.2. (THF), of analytical or HPLC grade. with grade 2 of ISO 3696. Apparatus as described A.2.3 Preparation of solutions See 8.7.3.3. THF can be substituted for acetone. An Internal Standard (1. S.) solution (8.7.3.3.4) is not required. Therefore, the NOTE addition of the 1.S. to the sample solutions (8.7.3.3.5) and the addition of the 1.S. to the calibration solutions (8.7.4.3.1) is not required. A.2.4 High performance liquid chromatography (HPLC) A.2.4.1 Reagent See 8.7.4.1. A.2.4.2 Apparatus A.2.4.2.1 High performance liquid chromatography, with ultraviolet spectroscopy detector capable of measuring at 205 nm and a recording system. A.2.4.2.2 A.2.4.3 Injection loop, of capacity e.g. 20 PI. Preparation of calibration solutions for acetone. See 8.7.4.3.1, except that 1.S. is not required and THF can be substituted 25 - IS ISO 6887:2005 1567:1999 HPLC chromatographic equipment and operating conditions: A.2.4.4 a) b) c) d) e) Column: Octadecyl silanized, 5 pm pore size, 250 mm length and 4 mm to 5 mm internal diameteh mobile phase: flowrate: detection: temperature: 66 % CH30H/3470 H20, isocratic elution; 0,8 ml/min; UV wavelength 205 nm constant room temperature NOTE The operating conditions can be altered if satisfactory separation is achieved. A different mobile phase system, e.g. acetonitrile/water (CH3CN/H20), can be used if separation is satisfactory. A.2.4.5 HPLC chromatograms of sample and calibration solutions The wavelength of 205 nm is suitable for low concentrations of MMA in the sample solution. The calibration graph shall be linear. If the concentration of the sample solution is too high, quantitative dilution of sample and calibration solutions is required, or a different choice of wavelength, e.g. 225 nm, can be made. To ensure that a constant volume of the sample solutions and the calibration fixed volume (e.g. 20 pl ) is used. solutions are injected, a loop with a To ensure correct quantification of the MMA content in the sample solutions, good separation of all substances be secured by selecting an appropriate mobile-phase composition. Operate the HPLC until all components A.2.4.6 Evaluation are completely eluted. shall of peaks from HPLC chromatograms and The retention time of MMA shall be known and shall be stable during the analyses of sample solutions calibration solutions. The retention time is dependent upon the column and mobile-phase composition. The peak height or area of MMA shall be determined by electronic registration and integration. A.2.5 A.2.5.1 A.2.5.1.1 Calculation and expression of results Calculation of results from a calibration graph graph in the calibration Drawing of the calibration Draw a calibration graph by plotting the peak area (or height) of methyl methacrylate monomer solution against the respective concentrations of MMA expressed in micrograms per milliJitre. A.2.5.1.2 Precision of measurements coefficient of the calibration graph established of the percentage The correlation A.2.5.1.3 by linear regression shall be not less than 0,990. Determination of methyl methacrylate of MMA (~MA) in the analysed sample solutions, in Use the calibration micrograms graph to determine the concentration per millilitre. Total quantity of MMA in the sample solution, mMMA (pg), is calculated as in 8.7.5.1.3. A.2.5.2 Expression of results See 8.7.5.3. 26 IS 6887:2005 ISO 1567:1999 Annex B (informative) Bibliography [1] ISO 10993-1:1992, Biological evacuation of medical devices -- Part 1: Guidance on selection of tests. Preclinica/ evaluation of biocompafibility of medical devices used in dentistry -- [2] ISO 7405:1997, Dentistry ­ Test methods for dental materials. 27 IS 6887:2005 ISO 1567:1999 AMENDMENT 1 Page 1, Scope Add to paragraph 1.1 Furthermore, it applies to denture base polymers for which the manufacturer claims that the material is a high impact polymer. It also specifies the requirement and the test method to be used. Page 1, Normative Add the following ISO 179:1993, references reference: of Charpy impact strength Plastics -- Determination 5.1.3 Page 4, subclause First line, delete Type 1 class 2 arid Type 2 class 2. Page 5, subclause Last paragraph, 5.2.10 `%. last line after 0,2 add "mass fraction". After subclause 5.2.12 add the following subclause: 5.2.13 Impact strength claims that the materied is a high impact polymer, the impact strength shall not be less When the manufacturer than 2,0 kJ/m2 when tested in accordance Page 14, subclause 8.5.3.5.2.5 with 8.9. Before 5.2.7 and 5.2.8 add "requirements of'. Page 16, subclause 8.7.3.3.2 Replace 8.7.3 .1.1.1 with 8.7.3.1.1. Page 22, subclause Second paragraph 8.8.5.4 replace two with three to read: "If at least three of the". After subclause 8.8.5.5 add the following subclause: 28 IS 6887:2005 ISO 1567:19$39 8.9 8.9.1 Impact strength Materials This consists of two specimen plates, freshly formed and processed in accordance with the manufacturer's instructions, each from a separate mix. Use the material, the apparatus (8.5.1.1) and the mould (8.5.1.1 .2) (except that the dimensions of the plates shall be (50 f 2) mm long, (50*2) mm wide and (4* 0,2) mm in height). 8.9.2 8.9.2.1 Apparatus See 8.5.3 .2.1,8.5.3.2.2 and 8.5.3.2.4. 8.9.2.2 Standard metallographic grinding papers, progressively approximately 26 pm (600 FEPA) for the final finishing stage. 8.9.2.3 Containers conditioning. 8.9.2.4 8.9.3 Pendulum Procedure of water, for storing the specimen finer grades using a grain size of strips at (23*2) "C and (37* 1) "C for pre-test impact testing machine, conforming to ISO 179:1993. A test capacity of 0,5 J is suitable. Within (24 +2) h of the beginning of the curing cycle of the denture base polymer, cut each plate lengthways into seven to eight equal strips, (50 f 2) mm long (/), (6* 0,2) mm wide (w) and (4* 0,2) mm in height (h). Machine the strips in a milling machine (8.5.3.2.2) on the edges and equally from both moulded surfaces so that the dimensions remain slightly oversized. Take care to avoid overheating the specimen strips. Wet-grind all faces and edges smooth and flat with metallographic grinding papers (8.9.2.2). Cut a notch (type A) (see Figure 4) in the middle of each specimen strip as described in ISO 179:1993. Cut the notch edgewise to a depth of (1,2* 0,1) mm leaving a residual depth beneath The radius of the notch base (tip) shall be (0,25* 0,05) mm (see Figure 5). the notch of (4,8* 0,1) mm. Iwl a b Direction of blow. See Figure 5. Figure 4 -- Charpy edgewise impact test, with single-notched specimen 29 IS ISO 6887:2005 1567: 1999 45° *l" Radius of notch base rn = (0,25 + 0,05) mm. Figure 5 -- Part of single-notched Measure residual specimen strip with type A notch and record, the height, h, [nominai (4A 0,2) mm] of each specimen strip near the notch and the depth, b, [nominai (4,8+ 0,1 ) mm] beneath the notch using a measuring instrument (8.2.1.5 or 8.5.3.2.4). Use only specimen strips which are of good quaiity and fail within the correct size range. Store 12 seiected specimen strips in the container of water at (37* 1) "C for 7 d * 2 h. Condition the specimen strips in the container of water at (23 t 2) "C for (60+ 15) min prior to testing. After conditioning, remove a specimen strip from the water and piace it on the specimen suppotts of the testing apparatus (8.9.2.4). Set the specimen supports at a separation of (40,0* 0,2) mm. Place the specimen strip with the notch facing away from the point of impact of the pendulum. Ensure that the specimen strip is centred with regard to the position of the notch and the point of impact of the penduium. As soon as possibie after removing each separate specimen strip from the water bath, release the penduium in order to fracture the specimen. Record the vaiue of energy absorbed, JI. Re-zero the instrument and aliow the penduium to swing again with no specimen recorded, .12, gives an indication of the friction in the system.) strip in place. (The energy 8.9.4 Calculate Caicuiation the impact and expression strength of resuits specimen, a, of notched in kilojoules per square metre (kJ/m2) using the formula: (J1-+103 bh where J, is the value of energy, in joules, absorbed by the specimen strip; J2 h is the friction energy, in joules, of the system; is the height, in millimetres, of the specimen strip; b is the depth, in miilimetres, behind the notch. 30 IS 6887:2005 ISO 1567:1999 8.9.5 Pass/fail determination of impact strength If results obtained for at least nine of the twelve specimen strips conform to the requirement stated in 5.2.13, the material fulfils the requirement of a high impact denture base polymer. If five or fewer of the twelve specimen strips conform to the requirement stated in 5.2.13, the polymer fails. If only six to eight of the twelve specimen strips conform to the requirement stated in 5.2.13, repeat the test. If at least ten of the second series of specimen strips conform to the requirement stated in 5.2.13, the polymer passes. 8.9.6 Expression of results evaluated, all results for impact strength with the number of specimens Report the number of specimens conforming to 5.2.13 and whether the material passes. Page 22, After subclause 9.2.1 k) add the following item: 1) the term "high impact" if the manufacturer wishes to claim that the material is a high impact polymer. If claimed, the polymer shall conform to the requirement of 5.2.13 when tested in accordance with 8.9. Page 23, After subclause 9.2.2 k) add the following item: 1) the term "high impact" if the manufacturer wishes to claim that the material is a high impact polymer. If claimed, the polymer shall conform to the requirement of 5.2.13 when tested in accordance with 8.9. Page 24, After subclause 9.3 m) add the following item. n) the term "high impact" if the manufacturer wishes to claim that the material is a high impact polymer. If claimed, the polymer shall conform to the requirement of 5.2.13 when tested in accordance with 8.9. 31 (Continued from second cover) The Technical Committee responsible the following International Standards for the preparation of this standard has reviewed the provisions of and has decided that they are acceptable for use in conjunction with this standard: International Standard Dial gauges reading Title in 0.01 mm, 0.001 in. and 0.0001 polymer teeth use -- Specification and test methods interchange -- in. lSO/R 463:1965 ISO 3336:1993 ISO 3696:1987 1s0 8601:2000 Dentistry -- Synthetic Water for analytical laboratory Data elements and interchange formats Representation of dates and times -- Information For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS 2 : 1960 `Rules for rounding off numerical values (revised)'. 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